Process for the recovery of aluminum chloride from the residue of aluminum chloride oil refining



Dec. 8, 1931 CARL ET AL 1,835,279

PROCESS FOR THE RECOVERY OF ALUMINUM CHLORIDE FROM THE RESIDUE OF ALUMINUM CHLORIDE OIL REFINING Filed Jan. 14, 1927 Patented Dec. 8, 1931 UNITED i.lfslrarss PATENT oFFIcE BYRON VGARLHOFNEW your. N.: A D wmmm s; AUSTIN, or NEWARK, EW JERSEY, ASSIGNORS mo ALUMIN M ouromnn OIL nrirINI GconroNArIo or NEW YORK, N. Y.,.A CORPORATION or DELAWARE PROCESS FOR 'rHEaEcovERY or ALUMINUM CHLORIDE FROM THE RESIDUE or K 1 AnuMINUrr CHLORIDE OIL REFINING r Application" filed Jenner-7 14, 1927. Serial No. 161,078.; a I

"This invention relates to an improvement in a process for therecovery of aluminum chloride from-the, residue of'aluminum chloride oil refining and. its novelty, .lies in the hereinafter pointed out. 1 V

In the refining of oil where aluminum chloride is used asxthe catalyst there comes a time when the Continuous process of. feedmg 011 andalumlnum chloride into the refining still must cease because of the accumu' lation' of a large quantity ofsludge which so impedes the progress of'refining that'i't is uneconomical .to proceed further; .The point at which this occurs varies, with'theeificien'cy of the various processes used; but the final result is-always the same in the:aluminum chloride oil refining processes and the sludge resulting is largely carbon in which the aluminum chloride is locked up and there is also some heavy oil residue combined therewith. This sludge, however, can'be broken up in the bottom of. the still and taken damn a more or less cokey condition-when the still iscleaned. is

Our process is adapted to take this'sludge which results at the end of a continuous 'oper-' ation in refining mineral oll with aluminum chloride and by grinding and regrinding said sludge until it ispulverized to the finestv form obtainable and carrying out this PIOCGSSrlli a drum maintained at a temperature sulficient to drive oif thealuminum chloridetrso exposed to thereby recover all or substantially allof the aluminum/chloride which is enmeshed or bound into the carbon or sludge,

thereby recovering the aluminum chloride for reuse in the distillingof mineral oil and,si-'

multaneously drawingoff from said sludgeany oil residue which may bebound therein. Our process therefore makes possible the economic recovery of the aluminum chloride which becomes bound into the sludge of the residue resulting from the distilling of mineral oil in the use of aluminum chloride as the catalyst. It also serves to recover any oil and pure carbon which are also bound in such sludge or residue making them both available for commercial use. r

The most desirable agent for the recovery more fully ofa high percentage' of low boiling oils of desired quality from mineral oil is aluminum ride combined with-the tremendous loss of unused aluminum chloride in the sludge resulting from all such distilling processes. has made the use of aluminum chloride unecon'omical in competition with other distilling processesin which aluminum chloride is not used. Our process infu-rnishing a means of recovering all or substantially all ofthe alu sideelevation of our complete apparatus for carrying out our-process,- certain portions tratiornf V Figure 2 is aperspective in detail of one of the crushing and .feeding arms.

In the drawings 3 is afurnace of usual construction having 'a frame 4 rigidly secured thereonat 14: in-Qtheusual and well known being broken awayfor convenience in illusmannerand an outer-frame portion. 5 also rigidly secured to thetop ofthefurnace 3 at 12' in the'usual well known manner so that a bearing Gatthe head-Of the same is' in alignment-with bearings 7, and 8;of offset bearing frames 9 and 10 rig-idly secured to the frame l in the usual well'kno'wn manner at 11. A 'drumcr cylinder-13 is rigidly secuied between vbase plates 15 andlfi of said; offset bearing frames 9 and 10.1 c.

shaft 17 is mounted in said and 8 so as to rotate freely therein a'ndfon the outer end of said shaft 117 ismountedin the usualwell known manner a pulley 18of usual construction and a belt connection to. a source of power (not shown), this being of usual Well known construction. A pipe 19 is rigidly {secured to one endgof the "drumz13 and at the I upperiend of said pipe 19 is rigidly. secured a feed hopperQO'in-which' is mounted a suitable feeding mechanism 21 of usjualconstruct ion adapted tofeed the sludge or residuein ;.ch'loride but the high cost of aluminum-chloiii) an even and continuous manner. A control valve 22 of usual construction is mounted in the pipe 19 below the feed hopper 20. At the opposite end of the drum 13 from pipe 19 is rigidly mounted a second pipe 23 having a control valve 24 of usual construction and terminating in a condensing chamber 25 of usual construction and to the upper side of said condenser 25 is rigidly secured a pipe 26 adapted to carry off the aluminum chloride to a suitable receptacle (not shown). The lowest point in the condenser 25 terminates in a pipe 27 which is adapted to lead to an oil receiving or containing means (not shown) to catch the oil condensed in said condenser 25. A pipe 28 is rigidly secured to the bottom of the drum 13 directly opposite pipe 23 and is adapted to take off into the receiving receptacle 29 to which said pipe 28 is secured all of the carbon and other residue which may remain at the end of the process described herein.

The portion of the shaft 17 lying within the drum13 is preferably of a hexagonal shape and a series of eccentric crushing and pushing arms 30 having hexagonal openings therethrough at 31 are adapted to be mounted thereon in a continuous staggered relation and said eccentric crushing and pushing arms 30 have lip portions 32 which serve to push the sludge or residue slightly forward on each revolution and these are arranged so as to point towards the exit or pipe 28 and faces 33 of said arms 30 are the crushing faces which as they'rotate are so close to the inner surface of the drum 13 all the way around that any sludge or residue material being treated lying within the range of their rotation is crushed and rolled between said faces 33 and the inner side of the drum 13.

In carrying out our process the sludge or residue from the aluminum chloride oil refining process is dumped into the feed hopper 20 and as the furnace 3 is infull operation, heating the drum 13 to the temperature necessary to drive off the aluminum chloride from said residue, the shaft 17 is put into operation by means of the application of power to the belt (not shown), running over the pulleylS whereby the shaft 17 and the eccentric crushing and pushing arms 30 will be rotated continuously always maintaining their staggered relation'as mounted on the shaft 17 and as the residue comes down the pipe 19 into the drum 13, said sludge or residue will be crushed by the faces 33 of the eccentric arms 30 against the inner wall of the drum 13 and upon each rotation of each of the arms 30 the lips 32 will serve to push forward a slight portion of the residue or sludge so that said sludge or residue will be crushed by each of the arms 30 a number of times before it is fed forward to the next arm 30 which will crush it still further whereby the sludge or residue will be pulverized to the finest form during its travel through the drum 13 and all-or substantially all of the aluminum chloride vapor and solid bound in said sludge or residue will be released and the aluminum chloride vapor is thereby exposed mechanically the heat at which the drum 13 is maintained will drive off said aluminum chloride and the same will be carried out through the pipe 23 through the chamber 25 and through pipe 26 to a suitable container at the end of pipe 26 (not shown).

As the residue being treated is pushed forward and crushed and recrushed many hun dreds of times before it finally reaches pipe 28, all. or substantially all of the aluminum chloride in said residue has a full opportre nity to be exposed to the heat in the drum 13 whereby it will all be driven off as described and simultaneously the oil which may be in said sludge or residue will also be driven ol'l' by the heat of said drum l3 and will pass off through pipe 23 and be condensed in condenser 25 and drawn off through pipe 27 into the container (not shown). The portion of the residue or sludge which has not been driven off by the heat in the drum 13 as it reaches the pipe 28 will fall down through said pipe into the container 29 and will be substantially a pure carbon free from oil and aluminum chloride.

It is quite apparent that many variations may be made in the apparatus disclosed without departing from the spirit and intent of our invention and that our process may be carried out by any such suitable apparatus.

We claim:

A process for the recovery of aluminum chloride from the residue of aluminum chloride oil refining comprising continuously feeding said residue into a drum, crushing and recrushing said residue continuously while passing slowly through said drum, maintaining a temperature throughout said drum sufficient to drive off all the aluminum chloride from said crushed residue and collecting the 1 same. a

In testimony whereof we aliix our signa- 

